Process for the preparation of water-soluble hydrocarbon derivatives.



m TED. STATES PATENT OFFICE.

FRIEDRICH BOLEG, OF CANNSTATT, GERMANY, ASSIGNOR TO GESELL- SCHAFT ZUR VERWERTUNG DER BOLEGSCHEN 'ASSERLOSLICHEN MINEBALOLE UND KOHLENWASSERSTOFFE, GESELLSCHAFT Mi'l BF- SCHRANKTER HAFTUNG, OF BERLIN, A CORPORATION OF GERMANY.

PROCESS FOR THE PREPARATION OF WATER-SOLUBLE HYDROCARBON Specification of Letters Patent.

CERlMTlVESf Patented April 23, 1907.

Application filed March 8,1904. SerialNo. 197,170. s.

To all whom, it may concern.-

Be it known that I, FRIEDRICH BOLEG, chemist, a subject of the King of Wiirtember residing at Cannstatt, in the Kingdom of Wiirtemberg, Germany, have invented a certain new and useful Improvement in Processes for the Preparation of Water-Soluble Hydrocarbon Derivatives; and I do hereby declare the following to be a full, clear, and exact description of the invention, such as will enable others skilled in the art to which it appertains to make and use the same.

The subject of the present invention consists of a process for the preparation of watersoluble or easily and permanently emulsifiable hydrocarbon derivatives, especially of aromatic hydrocarbons-such, for instance, as nitrobenzol, phenol, cresol, &c.

For the preparation of these hydrocarbon derivatives there are preferably used as the basis miscible or water-soluble mineral oils.

To render the mineral oils soluble in water, they are treated with crude rosin-oil and are then subjected to a washing and treatment with direct steam and caustic-soda solution in excess, whereupon the resutling alkaline mixture with oil after the separation of the rosin soap-lye is subjected to an oxidation process by the introduction of air under pressure or of ozone, and finally undergoes a shorter or longer treatment under a pressure of from one to one and a half atmospheres at temperatures which correspond to this ste am-pressure. The method of obtaining these watersoluble oils is described more in detail in my application Serial No. 126,273.

The hydrocarbon derivatives are treated at a temperature of from 40 Celsius, rising slowly to Celsius for about half an hour, with finely-divided air under pressure or ozone. At the same time for the purpose of saponifying the same so far as this is necessaryand desirable two to five per cent. of caustic-soda solution of 20 Baum in finelydivided condition is introduced, and to make up for the water evaporated about two per cent. more hotwater is introduced. The hydrocarbon derivatives thus treated are then, according to the kind and quality, intimately mixed with the water soluble mineral oil, which serves as a basis, andpreferably with the further addition of air under pressure. The application of air under pressure is also againuseful here in order to compensate for the. oxy gen escaping during the process from the oil mixture. H ereupon the preparation is cooled; but if it becomes cloudy it may be boiled for onehalf to one hour at a pressure of one-half to one atmosphere, the product being cooled.

Instead of using water-soluble m neral oils water-soluble rosin-oils may be sub ".itu ted a basis for mixture with the treated hydrocarbon derivatives. The method of produc-' ing such oils may be briefly described as follows: The crude oil is boiled with an excess of caustic-soda solution and with the direct application of steam, after which the alkaline mixture containing the rosin-oil is subjected to treatment with air under pressure or ozone at a temperature of from 95 to 110 Celsius until a clear solution is obtained.

As a specific example of the application of the invention the preparation of water-soluble nitrobenzol may be given as follows: One hundred parts of crude nitrobenzol or sixty-five parts of rectified nitrobenzol are heated in the air-pressure apparatus to about 50 Celsius, about from two to five per cent. ofsoda-lye and a little water added, and the whole mixed intimately for from fifteen to twenty mintues by passing air through it. There is then added seventy to eighty parts of the Water-soluble mineral or rosin oil heated to from 40 to 50 Celsius and allowed toilow in a thin stream and then heated to about Celsius, after which the air-supply is shut off and the mixture allowed to cool.

The water contents of the added mineral or rosin oil is proportionate to the purpose. of use in view and varies from fifteen to thirty per cent. The thirty or twenty per cent. nitrobenzol is specially intended for the pur pose of soap-making. If it, for instance, is required also as a domestic disinfectant, then a Weaker solution may be employed. It should be noted that it is only needful to use soda-lye when high-percentage compounds are to be produced.

What I claim, and desire to secure by Let-- ters Patent, is

1. The process of forming Water-miscible products from immiscible hydrocarbon (lesame with a water-soluble mineral oil.

2. The process of forming water-miscible products from immiscible hydrocarbon derivatives, which consists in air-blowing the same while in a heated state, and then incorporating the same with a water-soluble oil.

3. The process of making water-soluble hy- (lrocarbon derivatives, which consists in oxidizing a hydrocarbon derivative by submitting it to the action of oxygen while in a heated state, mixing with a water-soluble oil under the influence of air under pressure, and heating.

4. The process of making water-soluble hydrocarbon derivatives, which consists in oxidizing a hydrocarbon derivative by submitting it to the action of oxygen while maintainin the same at a temperature of 40 to elsius, mixing with a water-soluble oil under the influence of air under pressure, and heating.

5. The process of making water-soluble hydrocarbon derivatives, which consists in adding to a hydrocarbon derivative finelydivided alkalinesolution, subject-ing to the action of finelydivided gaseous oxygen while maintaining the same at a temperature of 40 to 60 Celsius, and mixing wlth a Watersoluble mineral oil by agitation with air under pressure whil heate 6. The process of making water-soluble hydrocarbon derivatives, which consists in adding to a hydrocarbon derivative two per cent. to five per cent. finely-divided causticsoda solution, blowing into the same gaseous oxygen while maintalning .a temperature of 40 to 60 Celsius, and mixing with seventy per cent. to eighty percent. of a water-soluble mineral oil by agitation with air under pressure, while maintaining a temperature of approximately Celsius.

7. The process of making water-soluble nitrobenzol which eonsists'in adding to nitrobenzol two per cent. to five per cent. causticsoda solution, agitating with gaseous oxygen under'pressurewhile maintaining a temperature of about 50 Celsius, adding seventy per cent. to eighty per cent. of wateresoluble mineral oil at a temperature of 40 to 50 Celsius, under agitation with air, and heating to a temperature of about 70 Celsius.

8. The process of making water-soluble hydrocarbon derivatives, which consists inoxidizing a hydrocarbon derivative by submitting it to the action of oxygen while maintainin the same at a temperature of 40 to 60 elsius, mixing with a water-soluble oil under the influence of air under pressure, heating, and boiling.

9. The process of making water-soluble hydrocarbon derivatives, which consists in adding to a hydrocarbon derivative finelydivided gaseous oxygnwhile maintaining the same at a temperature of 40 to 60 Cel- 'sius, mixing with a water-soluble mineral oil I under a pressure of one-half to one atmos- .phere.

In wltness whereof I have hereunto set my hand in presence of two Witnesses.

FRIEDRICH BOLEG.

Witnesses:

ARTHUR VoGT, RICHARD SEL NDEN. 

